The Preparation of Tetranitromethane
NORTHWESTERN UNIV EVANSTON IL
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Of the many methods for the preparation of TNM, the reaction between acetic anhydride and nitric acid seems the most promising. The reaction is best carried out in all-glass equipment consisting of a flask, mechanical sstirrer, dropping funnel, thermometer and condenser. Commercial fuming nitric acid can be used with success, but the yield of TNM is higher if the nitric acid is purified by vacuum distillation. No advantage is gained in purifying the acetic anhydride. The optimum temperature of reaction is 20-25 deg C, and the yield is enhanced by the presence of chipped glass. The yields of a considerable number of experiments averaged 61 to 62.
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